Nanocomposites of TiO2 Degussa P25 nanoparticles/activated carbon (TiO2/AC ) were prepared at various mass ratios of (4:1), (3:2), (2:3), and (1:4) by a facile process. The effects of TiO2/AC mass ratios on the structural, morphological, and photocatalytic properties were systematically studied in comparison with bare TiO2 and bare AC. TiO2 nanoparticles exhibited dominant anatase and minor rutile phases, and a crystallite size of approximately 21 nm; while AC had XRD peaks of graphite and carbon, and a crystallite size of 49 nm. The composites exhibited tight decoration of TiO2 nanoparticles on micron-/submicron AC particles, and uniform TiO2/AC composites were obtained as evidenced by the uniform distribution of Ti, O, and C in an EDS mapping. Moreover, Raman spectra show the typical vibration modes of anatase TiO2 (e.g., E1g(1), B1g(1), Eg(3)) and carbon materials with D and G bands. The TiO2/AC with (4:1), (3:2), and (2:3) possessed higher reaction rate constants (k) in photocatalytic degradation of methylene blue (MB) than that of either TiO2 or AC. Among the investigated materials, TiO2/AC = 4:1 achieved the highest photocatalytic activity with a high k of 55.2×10-3 min-1 and an MB removal efficiency of 96.6% after 30 min treatment under UV-Vis irradiation (120 mW/cm2). The enhanced photocatalytic activity for TiO2/AC is due to the synergistic effect of the high adsorption capability of AC and the high photocatalytic activity of TiO2. Furthermore, TiO2/AC promotes the separation of photoexcited electron/hole (e-/h+) pairs to reduce their recombination rate and thus enhance photocatalytic activity. The optimal TiO2/AC composite in this study can be used for treating industrial or household wastewater with organic pollutants.